微波辅助萃取-低温分配净化-气相色谱/质谱法同时检测土壤中63种持久性有机污染物  

Simultaneous determination of 63 persistent organic pollutants in soil by GC/MS with microwave-assisted extraction and low-temperature partition extraction purification

作　　者：黎玉清 赵波 金梦 闫雅楠 丁紫荣 李彦希 LI Yuqing;ZHAO Bo;JIN Meng;YAN Yanan;DING Zirong;LI Yanxi(South China Institute of Environmental Science,Ministry of Ecology and Environmental,Guangzhou,510655,China)

机构地区：[1]生态环境部华南环境科学研究所,广州510655

出　　处：《环境化学》2022年第12期4118-4129,共12页Environmental Chemistry

基　　金：中央级公益性科研院所基本科研业务专项(PM-zx703-202011-326);国家重点研发计划《粤港澳大湾区污染场地安全利用保障技术与集成工程示范》(2019YFC 1803900)资助.

摘　　要：建立了土壤中18种多氯联苯、23种有机氯农药、16种多环芳烃和6种邻苯二甲酸酯同时实验处理和仪器测定的分析方法.10.0 g土壤样品经30 mL正己烷+丙酮(1+1)试剂于110℃微波萃取15 min,萃取液氮吹浓缩到0.5 mL后于−20℃保持4 h进行低温分配净化,使用气相色谱-质谱法进行测定.结果显示,63种化合物的方法检出限在0.1—2.2μg·kg^(−1)之间,测定下限在0.4—8.8μg·kg^(−1)之间;对两个浓度水平的土壤基质加标样品分别进行6次平行分析,测定结果的回收率在76%—119%之间,相对标准偏差在0.4%—10.6%之间.对相关土壤标准物质进行分析,测定结果均在化合物质控范围内.研究表明本方法快速简便,回收率高,重现性好,能满足土壤中63种POPs的检测要求.与常规的前处理净化相比,该方法操作简单,具备批处理优势,在分析大批量样品时,可提高工作效率,节省监测成本.A method for simultaneous determination of 18 PCBs,23 OCPs,16 PAHs and 6 PAEs in soils by gas chromatography-mass spectrometry(GC-MS),with microwave extraction and lowtemperature partition extraction purification was developed.Microwave-assisted extraction conditions involved the use of 30 mL n-hexane+acetone(1+1)at 115℃for 5 min,the collected extraction liquid was concentrated to 0.5 mL by nitrogen,and subsequently in a freezer at−20℃for 4 h.After the water phase was iced,the upper organic phase was taken out and analyzed by GC-MS.The result shows that,detection limits of this method were 0.1—2.2μg·kg^(−1),quantitative lower limits were 0.4—8.8μg·kg^(−1),and average recoveries of spiked samples ranged from 76%to 119%with relative standard deviations between 0.4%and 10.6%.The determination results of soils standard reference materials were all in the acceptance limits.The method shows high accuracy and precision,fast simple operation,high throughput and suitable for the simultaneous determination of 63 persistent organic pollutants(POPs)in the soil.

关 键 词：微波辅助萃取 低温分配 持久性有机污染物 高通量分析方法 

分 类 号：O657.63[理学—分析化学] X833[理学—化学]